CN111995864A - Polyamide composition and preparation method thereof - Google Patents
Polyamide composition and preparation method thereof Download PDFInfo
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- CN111995864A CN111995864A CN202010703696.XA CN202010703696A CN111995864A CN 111995864 A CN111995864 A CN 111995864A CN 202010703696 A CN202010703696 A CN 202010703696A CN 111995864 A CN111995864 A CN 111995864A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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Abstract
The invention provides a polyamide composition and a preparation method thereof, wherein the composition is prepared from the following raw materials in parts by weight: 57-88 parts of polyamide resin, 10-30 parts of polyetherimide, 1-5 parts of poly (arylene ether nitrile), 1-5 parts of compatilizer, 0.1-0.5 part of heat stabilizer and 0.1-1 part of processing aid. The polyamide composition disclosed by the invention has excellent flame retardant property, the limited oxygen index reaches more than 32, and meanwhile, the polyamide composition has good transparency and heat resistance.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a polyamide composition and a preparation method thereof.
Background
Polyamide (PA), also known as nylon, was commercialized in 1939. With the development of industrial technology, transparent nylon is gradually applied to the market, has the inherent characteristics of nylon, including mechanical property, heat resistance, abrasion resistance, chemical resistance and self-lubrication, has low friction coefficient, is easy to process, is suitable for being filled with glass fiber and other fillers for reinforcing and modifying, but cannot achieve the transparent effect after reinforcing and flame-retardant modification in some special fields, so that the application of the transparent nylon is limited.
The polyetherimide is an amber transparent high polymer material and has high temperature resistance, solvent resistance, radiation resistance, hydrolysis resistance, flame retardant property and the like. The excellent performance enables the application range to be wider, for example, some parts with higher temperature resistance are manufactured, the excellent electrical insulation performance can be applied to the field of electronics and electricity, the use temperature is 180-200 ℃, and the injection molding temperature is 330 ℃. In particular, the good flame retardant property of the flame retardant is applied to some service environments with fire prevention requirements.
In the fields of security, mineral production, oil exploitation and the like, for the requirement of safety, high temperature resistance and the requirements of transparency and fire resistance are required under certain high-temperature environments, the traditional flame-retardant material is adopted, the traditional flame-retardant material is not high in heat resistance, most of the fireproof materials are opaque, the polyetherimide material is adopted, the fireproof grade of the polyetherimide material can meet the requirements, but amber has certain influence on the transparency of the polyetherimide material, and the transparent nylon has good performances of oil resistance, heat resistance and the like and cannot meet the requirement of fire resistance, so that any one material used independently is difficult to meet the application of the current market. If the transparent nylon and polyetherimide material are used as alloy materials, the alloy material not only can meet the requirements of high heat resistance and fire resistance, but also has the unique performance advantage of transparency, and the alloy of the material is rarely reported at present.
Disclosure of Invention
In view of the above, the present invention provides a polyamide composition and a preparation method thereof, which aims to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a polyamide composition characterized by: the composition is prepared from the following raw materials in parts by weight:
preferably, the composition is prepared from the following raw materials in parts by weight:
further, the polyamide resin is transparent polyamide; the light transmittance of the polyamide resin is more than or equal to 90 percent; the polyamide resin is polyamide with the carbon chain length between adjacent amide groups being greater than or equal to 10.
Further, the polyetherimide is formed by condensation polymerization of bisphenol A type diether dianhydride and diamine monomer; the diamine is prepared by copolymerizing phenylenediamine and propane diamine, wherein the molar ratio of the phenylenediamine to the propane diamine is 1-4: 1. the polyamide resin is polyetherimide superfine powder.
Further, the polyarylether nitrile is amorphous polyarylether nitrile; the polyarylether nitrile is formed by the reaction and polymerization of at least one of bisphenol A, bisphenol S or phenolphthalein and 2, 6-dichlorobenzonitrile; preferably, the polyarylether nitrile is prepared by polymerizing phenolphthalein and 2, 6-dichlorobenzonitrile.
Further, the compatilizer is at least one of N-methyl pyrrolidone, dimethyl sulfoxide, N-dimethylacetamide or N, N-dimethylformamide; the compatilizer is N-methyl pyrrolidone. The N-methyl pyrrolidone enables the material to have high polarity and reactivity, and can greatly improve the compatibility of the composite material. The compatibilizer is the polar aprotic solvent.
Further, the heat stabilizer is cage-type polysilsesquioxane, the cage-type polysilsesquioxane is a nano-based polymer, the R end of the cage-type polysilsesquioxane is an organic side group, and the organic side group is at least one of methyl, hydroxyalkyl, aminoalkyl, phenolic group, pyridyl group, epoxy group, carboxyl group or acid anhydride group; the organic side group is pyridyl, phenolic group and acid anhydride group.
Further, the processing aid is at least one of an antioxidant or a coupling agent; the antioxidant is a compound of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylene diamine and bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite; the coupling agent is a silane coupling agent containing amino.
The preparation method of the polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the polyarylether nitrile, the heat stabilizer, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
Further, in the step (2), the temperature of the first zone of the twin-screw extruder is 250-minus 270 ℃, the temperature of the second zone is 260-minus 280 ℃, the temperature of the third zone is 260-minus 280 ℃, the temperature of the fourth zone is 260-minus 280 ℃, the temperature of the fifth zone is 270-minus 290 ℃, the temperature of the sixth zone is 280-minus 300 ℃, the temperature of the seventh zone is 270-minus 290 ℃, the temperature of the eighth zone is 260-minus 280 ℃, the temperature of the ninth zone is 240-minus 260 ℃, the retention time is 1-3 minutes, and the rotation speed of the host machine is 250-minus 350 revolutions per minute.
Reduction of the viscosity of Polyetherimide (PEI) with silicone oil: the PEI is filled with the hydroxyl silicone oil, the hydroxyl silicone oil can be combined with the viscous components in the PEI, even a clathrate compound is formed, so that the quantity of the viscous components of the PEI system is reduced, the viscosity of the PEI system is reduced, the reduced PEI is fully bonded with the silicone oil for later use at a certain temperature, and thus the subsequent dispersibility of the PEI and the nylon is facilitated, and the processability of the composition is improved.
Compared with the prior art, the invention has the following advantages:
the polyamide composition disclosed by the invention has excellent flame retardant property, the limited oxygen index reaches more than 32, and meanwhile, the polyamide composition has good transparency and heat resistance.
The polyamide composition provided by the invention adopts polyether aromatic nitrile as a high-performance polymer, so that the thermal stability of the composition is further improved, and the polyamide composition has good compatibility with a system.
The heat stabilizer in the polyamide composition is cage-type polysilsesquioxane, so that the optical performance and the flame retardant performance of the composition can be effectively improved.
The polyamide composition can be widely applied to the application fields with requirements on transparency, high heat resistance and fire resistance.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
In the examples and comparative examples described in the present invention: the polyamide resin is PA12, Trogamid CX series of Evonik company; selecting PEN ID 300 of Japan light from the poly (arylene ether nitrile); selection of Mitsubishi chemical for polyetherimides
U1000; the compatilizer is N-methylpyrrolidone (NMP); heat stabilizer selection pyridyl cageA type silsesquioxane; the antioxidant is IRGANOX1098 produced and sold by Ciba.
The present invention will be described in detail with reference to examples.
Example 1
The polyamide composition is prepared from the following raw materials in parts by weight: 75.6 parts of polyamide resin, 20 parts of polyetherimide, 1 part of poly (arylene ether nitrile), 3 parts of compatilizer, 0.1 part of heat stabilizer and 0.3 part of antioxidant.
The preparation method of the polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the polyarylether nitrile, the heat stabilizer, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 2
The polyamide composition is prepared from the following raw materials in parts by weight: 74.6 parts of polyamide resin, 20 parts of polyetherimide, 2 parts of poly (arylene ether nitrile), 3 parts of compatilizer, 0.1 part of heat stabilizer and 0.3 part of antioxidant.
The preparation method of the polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the polyarylether nitrile, the heat stabilizer, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 3
The polyamide composition is prepared from the following raw materials in parts by weight: 74.5 parts of polyamide resin, 20 parts of polyetherimide, 2 parts of poly (arylene ether nitrile), 3 parts of compatilizer, 0.2 part of heat stabilizer and 0.3 part of antioxidant.
The preparation method of the polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the polyarylether nitrile, the heat stabilizer, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 4
The polyamide composition is prepared from the following raw materials in parts by weight: 71.5 parts of polyamide resin, 20 parts of polyetherimide, 5 parts of poly (arylene ether nitrile), 3 parts of compatilizer, 0.2 part of heat stabilizer and 0.3 part of antioxidant.
The preparation method of the polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the polyarylether nitrile, the heat stabilizer, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 5
The polyamide composition is prepared from the following raw materials in parts by weight: 71 parts of polyamide resin, 20 parts of polyetherimide, 5 parts of poly (arylene ether nitrile), 3 parts of compatilizer, 0.7 part of heat stabilizer and 0.3 part of antioxidant.
The preparation method of the polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the polyarylether nitrile, the heat stabilizer, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Comparative example 1
The polyamide composition is prepared from the following raw materials in parts by weight: 79.6 parts of polyamide resin, 20 parts of polyetherimide and 0.3 part of antioxidant.
The preparation method of the polyamide composition comprises the following steps: the preparation method comprises the steps of uniformly mixing polyamide resin, polyetherimide and an antioxidant in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, cooling, drying and dicing after extrusion to obtain the polyamide resin.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
And (3) putting the prepared granules into a blast oven, drying for 4h at the temperature of 110 ℃, and then injecting the dried granules into an injection molding machine for molding sample strips. The injection molding mold temperature was 60 ℃. The performance test criteria of the polyamide compositions obtained according to the invention are shown in table 1.
Table 1 test items of physical and mechanical properties of materials and corresponding test methods
| Test items | Test method and conditions |
| Light transmittance | GBT 2410-2008/1mm |
| Limiting oxygen index | GB2406 |
| Heat distortion temperature | GB1634/ISO 75/1.82MPa |
| Glass transition temperature | GB19466 |
The physical properties of the polyamide compositions obtained in examples 1 to 5 and comparative example 1 are shown in Table 2.
TABLE 2 physical Properties of Polyamide compositions
| Test items | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 |
| Light transmittance | 83 | 85 | 88 | 90 | 93 | 83 |
| Limiting oxygen index | 35 | 36 | 37 | 39 | 41 | 35 |
| Heat distortion temperature | 95 | 98 | 99 | 102 | 105 | 90 |
| Glass transition temperature | 185 | 188 | 192 | 195 | 198 | 180 |
As can be seen from Table 2, the polyamide composition provided by the invention has excellent light transmittance, flame retardant property and heat resistance, can meet the transparent effect, can be used in some environments requiring perspective, has good combustion performance, can be applied to fields requiring high safety protection requirements such as mines and the like, has increased heat resistance, and better fills up the application blank that transparent materials are required in environments with high temperature of more than 220 ℃. Meanwhile, the polyamide composition can also be widely applied to the field of electronics and electrics.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A polyamide composition characterized by: the composition is prepared from the following raw materials in parts by weight:
2. the polyamide composition of claim 1, characterized in that: the polyamide resin is transparent polyamide; the light transmittance of the polyamide resin is more than or equal to 90 percent; the polyamide resin is polyamide with the carbon chain length between adjacent amide groups being greater than or equal to 10.
3. The polyamide composition of claim 1, characterized in that: the polyetherimide is prepared by condensation polymerization of bisphenol A type diether dianhydride and diamine monomer; the diamine is prepared by copolymerizing phenylenediamine and propane diamine, wherein the molar ratio of the phenylenediamine to the propane diamine is 1-4: 1.
4. the polyamide composition of claim 1, characterized in that: the polyarylether nitrile is amorphous polyarylether nitrile; the polyarylether nitrile is formed by the reaction and polymerization of at least one of bisphenol A, bisphenol S or phenolphthalein and 2, 6-dichlorobenzonitrile; preferably, the polyarylether nitrile is prepared by polymerizing phenolphthalein and 2, 6-dichlorobenzonitrile.
5. The polyamide composition of claim 1, characterized in that: the compatilizer is at least one of N-methyl pyrrolidone, dimethyl sulfoxide, N-dimethylacetamide or N, N-dimethylformamide; the compatilizer is N-methyl pyrrolidone.
6. The polyamide composition of claim 1, characterized in that: the heat stabilizer is cage-type polysilsesquioxane, the cage-type polysilsesquioxane is a nano-polymer, the R end of the cage-type polysilsesquioxane is an organic side group, and the organic side group is at least one of methyl, hydroxyalkyl, aminoalkyl, phenolic group, pyridyl, epoxy group, carboxyl or acid anhydride group; the organic side group is pyridyl, phenolic group and acid anhydride group.
7. The polyamide composition of claim 1, characterized in that: the processing aid is at least one of an antioxidant or a coupling agent; the antioxidant is a compound of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylene diamine and bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite; the coupling agent is a silane coupling agent containing amino.
8. Process for the preparation of a polyamide composition according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the polyarylether nitrile, the heat stabilizer, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
9. The method for preparing a polyamide composition according to claim 8, characterized in that: in the step (2), the temperature of the first zone of the twin-screw extruder is 250-.
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2020
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| US4657987A (en) * | 1984-01-27 | 1987-04-14 | General Electric Company | Polyetherimide-polyamide blends |
| US5013799A (en) * | 1984-01-27 | 1991-05-07 | Giles Jr Harold F | Polyetherimide-polyamide blends |
| CA1280238C (en) * | 1985-06-28 | 1991-02-12 | John Andrew Rock | Polyetherimide-polyamide blends |
| US5166246A (en) * | 1986-01-06 | 1992-11-24 | General Electric Company | Polyetherimide-polyamide compositions |
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